ES2199434T3 - CHEMICAL COMPOSITIONS. - Google Patents

CHEMICAL COMPOSITIONS.

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Publication number
ES2199434T3
ES2199434T3 ES98913569T ES98913569T ES2199434T3 ES 2199434 T3 ES2199434 T3 ES 2199434T3 ES 98913569 T ES98913569 T ES 98913569T ES 98913569 T ES98913569 T ES 98913569T ES 2199434 T3 ES2199434 T3 ES 2199434T3
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ES
Spain
Prior art keywords
indicator
component
components
weight
polyol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
ES98913569T
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Spanish (es)
Inventor
Christopher Victor Keen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huntsman Advanced Materials Switzerland GmbH
Original Assignee
Vantico GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vantico GmbH filed Critical Vantico GmbH
Application granted granted Critical
Publication of ES2199434T3 publication Critical patent/ES2199434T3/en
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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/0008Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0041Optical brightening agents, organic pigments

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Paints Or Removers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Immobilizing And Processing Of Enzymes And Microorganisms (AREA)

Abstract

Sistema de envase múltiple que comprende dos o metálic componentes que reaccionan conjuntamente para formar una resina termoendurecible, caracterizado porque uno de los componentes contiene hasta un 0,01% en peso de un indicador de pH.Multiple container system comprising two or metal components that react together to form a thermosetting resin, characterized in that one of the components contains up to 0.01% by weight of a pH indicator.

Description

Composiciones químicas.Chemical compositions

El presente invento se refiere a sistemas que reaccionan para producir resina termofraguante, comprendiendo el sistema un poliol en un componente y un isocianato como un segundo componente y hasta 0,01% en peso de un indicador de pH en uno de dichos componentes.The present invention relates to systems that react to produce thermosetting resin, comprising the system a polyol in one component and an isocyanate as a second component and up to 0.01% by weight of a pH indicator in one of these components.

Las resinas termofraguantes tal como poliuretanos y resinas epoxi se utilizan ampliamente, por ejemplo como adhesivos, para obtener revestimientos y en aplicaciones de herramientas. En muchos casos la mezcla de los componentes es muy similar en apariencia a algunos o todos los componentes individuales. Es por tanto posible producir productos en donde se omite uno o mas componentes, por ejemplo debido a la interrupción de la máquina, y pasar inadvertido al operario este evento.Thermosetting resins such as polyurethanes and epoxy resins are widely used, for example as adhesives, to obtain coatings and in applications of tools In many cases the mixing of the components is very similar in appearance to some or all components individual. It is therefore possible to produce products where omit one or more components, for example due to interruption of the machine, and pass this operator inadvertently.

En algunos casos se adiciona un colorante o pigmento a un componente y luego es posible asegurar la mezcla apropiada observando el color de la mezcla, y comparándolo con el color del componente individual. Esto requiere normalmente de 0,1 a 5% de costoso colorante o pigmento.In some cases a dye or pigment to a component and then it is possible to ensure the mixture appropriate observing the color of the mixture, and comparing it with the color of the individual component. This normally requires 0.1 to 5% expensive dye or pigment.

Hemos encontrado ahora, sorprendentemente, que una cantidad muy reducida de un compuesto que se utiliza normalmente como un indicador de cambio de pH, exhibe también un cambio de color en los sistemas termofraguantes.We have found now, surprisingly, that a very small amount of a compound that is used normally as an indicator of pH change, it also exhibits a color change in thermoforming systems.

Así pues, el presente invento proporciona un sistema multi-envase que comprende dos o mas componentes que reaccionan entre sí para formar una resina termofraguante, cuyo sistema comprende un poliol en un componente y un isocianato como un segundo componente y hasta 0,01% en peso de un indicador, caracterizado porque el indicador es un indicador de pH que produce un cambio de color cuando se mezclan los componentes y está presente en el componente poliol.Thus, the present invention provides a multi-container system comprising two or more components that react with each other to form a resin thermoforming agent, whose system comprises a polyol in one component and an isocyanate as a second component and up to 0.01% by weight of an indicator, characterized in that the indicator is an indicator of pH that produces a color change when the components are mixed and is present in the polyol component.

Usualmente el sistema del invento comprenderá dos envases, cada uno de los cuales contiene un componente reactivo.Usually the system of the invention will comprise two packaging, each of which contains a component reagent.

Solo se precisan cantidades muy pequeñas de indicador para producir un cambio de color deseado. Usualmente es suficiente menos de 0,01% en peso del componente al que se adiciona. De preferencia la cantidad se encuentra entre 0,0003% y 0,006%, y mas preferentemente entre 0,0005% y 0,004%.Only very small amounts of indicator to produce a desired color change. Usually is sufficient less than 0.01% by weight of the component to which add. Preferably the amount is between 0.0003% and 0.006%, and more preferably between 0.0005% and 0.004%.

El indicador puede adicionarse a cualquier componente siempre que no reaccione con dicho componente y así impedir el cambio de color.The indicator can be added to any component as long as it does not react with that component and so Prevent color change.

Muchos indicadores, tal como los que contienen uno o mas grupos fenólicos, reaccionarán con isocianatos con lo que se destruye el cromóforo. En este caso el indicador debe adicionarse al componente poliólico.Many indicators, such as those containing one or more phenolic groups will react with isocyanates with what The chromophore is destroyed. In this case the indicator must add to the polyol component.

Puede utilizarse cualquier indicador que produzca un cambio de color cuando se mezclan los componentes. Sin embargo el indicador es de preferencia uno que, en sistemas acuosos, empiece a cambiar el color por lo menos a un pH inferior a 8,2. Se prefieren especialmente aquellos que se colorean fuertemente en estados ácido y alcalino o aquellos que dan un fuerte color alcalino a valor pH bajos, por ejemplo inferiores a 5,0. Como ejemplos de indicadores apropiados puede citarse Cresol Red, Bromophenol Blue, Bromocresol Green, Bromocresol Purple, Chlorophenol Red, Phenol Red y Thymol Blue.Any indicator that produces a color change when the components are mixed. Nevertheless the indicator is preferably one that, in aqueous systems, Start changing the color at least at a pH below 8.2. I know they especially prefer those that are strongly colored in acid and alkaline states or those that give a strong color low pH alkaline, for example less than 5.0. How Examples of appropriate indicators can be cited Cresol Red, Bromophenol Blue, Bromocresol Green, Bromocresol Purple, Chlorophenol Red, Phenol Red and Thymol Blue.

Debe apreciarse que el cambio de color observado no es siempre el mismo en diferentes sistemas y no es también siempre el mismo que el cambio de color producido con el cambio del pH en un sistema acuoso. Por ejemplo Chlorophenol Red cambia de naranja a beige en sistemas poliuretánicos. Cuando se indica un cambio de pH el color cambia de amarillo a rojo.It should be noted that the observed color change it is not always the same in different systems and it is not also always the same as the color change produced with the change of pH in an aqueous system. For example Chlorophenol Red changes from Orange to beige in polyurethane systems. When a pH change the color changes from yellow to red.

Cuando se mezclan los dos componentes, la persona que lleva a cabo la operación puede ver fácilmente a partir del cambio de color que los dos componentes se han mezclado, y que la mezcla es uniforme a través de la mezcla.When the two components are mixed, the person who performs the operation can easily see from the color change that the two components have mixed, and that the Mix is uniform throughout the mix.

El invento se ilustra por medio de los ejemplos siguientes.The invention is illustrated by means of the examples. following.

Ejemplos 1-6Examples 1-6

Se prepara poliuretanos a partir de un componente poliólico (A) y el componente (B) que es 4,4'-metilen difenil diisocianato líquido semidestilado (MDI) en una relación de (A):(B) de 100:25 en peso. El componente (A) tiene la composición:Polyurethanes are prepared from a component polyol (A) and component (B) which is 4,4'-methylene diphenyl diisocyanate liquid semi-distilled (MDI) in a ratio of (A) :( B) of 100: 25 by weight. The component (A) has the composition:

         \newpage\ newpage
      

Componente poliólico - (A) Polyol component - (TO) % peso/peso% weight / weight Aceite de ricino BPOil of BP castor 32,132.1 Poliéter poliol ramificado - Peso equivalente 148 (Desmophen 55OU, de Bayer)Polyether polyol Branched - Equivalent Weight 148 (Desmophen 55OU, of Bayer) 13,913.9 DolomitaDolomite 49,049.0 Sílice ahumadoSilica smoked 2,02.0 Tamiz molecularSieve molecular 3,03.0

Se adicionan indicadores al componente (A) como una solución al 0,1% en un vehículo apropiado que es aceite de ricino o un poliol (Lupranol 1000, BASF). Se obtienen los resultados siguientesIndicators are added to component (A) as a 0.1% solution in an appropriate vehicle that is oil from castor or a polyol (Lupranol 1000, BASF). You get the following results

EjemploExample Indicador Indicator % peso/peso en el% weight / weight in Cambio de color con mezcla con elColor change with mixing with the comp. (A)comp. (TO) comp. (B)comp. (B) 1one Azul de bromofenolBromophenol blue 0,0030.003 Azul -> beigeblue -> beige 2two Verde de bromocresolGreen of bromocresol 0,0030.003 Verde -> beigeGreen -> beige 33 Púrpura de bromocresolPurple bromocresol 0,0030.003 Amarillo -> beigeYellow -> beige 44 Rojo cresolRed cresol 0,0030.003 Amarillo claro -> beigeLight yellow -> beige 55 Rojo de clorofeniloRed from chlorophenyl 0,0030.003 Naranja -> beigeOrange -> beige 66 Rojo fenolPhenol red 0,0030.003 Rosa claro -> beigepink clear -> beige

Ejemplos 7-9Examples 7-9

Siguiendo el procedimiento de los ejemplos 1-6 donde los ingredientes son como se expone a continuación, siendo MDI el componente (B) y el resto es el componente (A), obteniéndose el cambio de color con la adición de (B) a (A) como se ha expuesto.Following the procedure of the examples 1-6 where the ingredients are as exposed to then, being MDI the component (B) and the rest is the component (A), obtaining the color change with the addition of (B) to (A) as stated.

EjemploExample 77 88 99 N,N,N',N'-tetrakis(2-hidroxi-propil) etilen diamina(Quadrol "L",N, N, N ', N'-tetrakis (2-hydroxy-propyl) ethylene diamine (Quadrol "L", BASF)BASF) 3030 -- -- Poliéter poliol ramificadoPolyether polyol branched Peso equivalente 148 (Desmophen 550U, Bayer)Weight equivalent 148 (Desmophen 550U, Bayer) -- 4444 -- Aceite de ricino nº 1Castor Oil No. one -- -- 4444 Poliéter triol altamente reactivo (Lupranol 2042, BASF)Highly reactive triol polyether (Lupranol 2042, BASF) 6464 -- -- DolomitaDolomite -- -- 50fifty Carbonato cálcicoCarbonate calcic -- 50fifty -- Tamiz molecularMolecular sieve 33 33 33 Azul de timol (0,1% en Lupranol 1000)Thymol blue (0.1% in Lupranol 1000) 33 -- -- Azul, de bromofenol (0,1% en Lupranol 1000)Blue, bromophenol (0.1% in Lupranol 1000) -- 33 --

(Continuación)(Continuation)

EjemploExample 77 88 99 Verde de bromocresol (0,1% en Lupranol 1000)Bromocresol green (0.1% in Lupranol 1000) -- -- 33 MDI modificado (Lupranat MP 102, BASF)Modified MDI (Lupranat MP 102, BASF) 80,580.5 -- -- MDI semi-destilado (Lupranat M20S, BASF)Semi-distilled MDI (Lupranat M20S, BASF) -- 4040 -- MDI semi-destilado (Desmodur 44V20L, Bayer)Semi-distilled MDI (Desmodur 44V20L, Bayer) -- -- 1717 Cambio de colorChange of color Amarillo-Yellow- Azul-beigeBlue-beige Gris/verde-Gray / green- Crema/blancoCream / white beigebeige

Ejemplos 10-13Examples 10-13

Se utilizan diferentes cantidades de indicador en un sistema poliuretánico para mostrar los diferentes cambios de color. Los ingredientes utilizados y los cambios de color son como sigue:Different amounts of indicator are used in a polyurethane system to show the different changes of color. The ingredients used and the color changes are like follow:

EjemploExample 1010 11eleven 1212 1313 N,N,N',N'-tetrakis (2-hidroxipropil)etilenN, N, N ', N'-tetrakis (2-hydroxypropyl) ethylene diamina (Quadrol "L", BASF)diamine (Quadrol "L", BASF) 3030 3030 3030 3030 Poliéter triol altamente reactivo (LupranolHighly reactive triol polyether (Lupranol 6464 6464 6464 6464 2042, BASF)2042, BASF) Tamiz molecularSieve molecular 33 33 33 33 Azul de bromofenolBlue of bromophenol 0,0060.006 0,0010.001 0,00050.0005 0,00030.0003 MDI semi-destilado (Desmodur 44V20L,Semi-distilled MDI (Desmodur 44V20L, Bayer)Bayer) 5959 5959 5959 5959 Cambio de color de Azul intenso -> Azul muy claroColor change Intense blue -> Very light blue con adición de DMI a Azul claro -> Incolorowith addition of DMI to Light Blue -> Colorless

Claims (3)

1. Un sistema multienvase que comprende dos o mas componentes que reaccionan entre sí para formar una resina termofraguante cuyo sistema comprende un poliol en un componente y un isocianato como un segundo componente y hasta 0,01% en peso de un indicador en uno de dichos componentes, caracterizado porque el indicador es un indicador de pH que produce un cambio de color cuando se mezclan los componentes y está presente en el componente poliólico.1. A multipack system comprising two or more components that react with each other to form a thermosetting resin whose system comprises a polyol in one component and an isocyanate as a second component and up to 0.01% by weight of an indicator in one of said components, characterized in that the indicator is a pH indicator that produces a color change when the components are mixed and is present in the polyol component. 2. Un sistema de conformidad con la reivindicación 1, caracterizado porque la cantidad de indicador está comprendida entre 0,003% y 0,006% en peso.2. A system according to claim 1, characterized in that the amount of the indicator is between 0.003% and 0.006% by weight. 3. Un sistema, de conformidad con la reivindicación 1 y 2, caracterizado porque el indicador es Cresol Red, Bromophenol Blue, Bromocresol Green, Bromocresol Purple, Chlorophenol Red, Phenol Red o Thymol Blue.3. A system according to claim 1 and 2, characterized in that the indicator is Cresol Red, Bromophenol Blue, Bromocresol Green, Bromocresol Purple, Chlorophenol Red, Phenol Red or Thymol Blue.
ES98913569T 1997-03-26 1998-02-20 CHEMICAL COMPOSITIONS. Expired - Lifetime ES2199434T3 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GBGB9706223.6A GB9706223D0 (en) 1997-03-26 1997-03-26 Chemical compositions
GB9706223 1997-03-26

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ES2199434T3 true ES2199434T3 (en) 2004-02-16

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US (1) US6060544A (en)
EP (1) EP0970133B1 (en)
JP (1) JP2001518973A (en)
AT (1) ATE240358T1 (en)
CA (1) CA2284841A1 (en)
DE (1) DE69814604T2 (en)
ES (1) ES2199434T3 (en)
GB (1) GB9706223D0 (en)
ID (1) ID22634A (en)
TW (1) TW496888B (en)
WO (1) WO1998042762A1 (en)
ZA (1) ZA982513B (en)

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DE19928676A1 (en) * 1999-06-23 2000-12-28 Basf Ag Polyisocyanate poly-addition product, e.g. flexible polyurethane foam for cushions and padding, contains hydrophobic compounds and other special modifiers, e.g. metal salt, anhydride, sulfone or unsaturated acid
DE10115004A1 (en) * 2001-03-26 2002-10-10 Input Inst For Polyurethane Te Control of moisture induced curing of polyurethane foam with a pH indicator, useful for curing foamed assembly materials, adhesives, and jointing compounds ensures adequate curing by following the color change with increase in pH
DE102008019017B3 (en) * 2008-04-15 2009-12-31 Mankiewicz Gebr. & Co. Gmbh & Co Kg Curable compositions containing color indicators for indicating the curing progress and methods for indicating the curing progress of these curable compositions
US8975312B2 (en) * 2010-06-29 2015-03-10 3M Innovative Properties Company Color indicating epoxy resins and methods thereof
US20160151251A1 (en) * 2012-12-20 2016-06-02 Kao Germany Gmbh Aqueous oxidizing composition
JP2018502179A (en) 2014-11-18 2018-01-25 スリーエム イノベイティブ プロパティズ カンパニー Discoloring adhesive composition
CN112480370A (en) 2015-03-19 2021-03-12 泽费罗斯股份有限公司 Esterified acids for polymeric materials
KR102780994B1 (en) * 2018-02-22 2025-03-14 신에쓰 가가꾸 고교 가부시끼가이샤 Room temperature curable organopolysiloxane composition, structure and method for determining the curing state of the composition
JP7265242B2 (en) * 2018-12-10 2023-04-26 国立研究開発法人宇宙航空研究開発機構 RESIN COMPOSITION, METHOD FOR PREDICTING FAILURE OF CURE, METHOD FOR MANUFACTURING JOINTED BODY, ADHESION KIT, AND DETERMINATION OF DEFAULT-CUREMENT
AU2020256063B2 (en) 2019-04-03 2022-06-02 Zephyros, Inc. Two-part phosphate ester epoxy composition
CN118176229A (en) * 2021-10-29 2024-06-11 泽菲罗斯有限公司 Reaction-induced color-changing composition

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US3773706A (en) * 1971-11-26 1973-11-20 Ubm Armonk Method for indicating stage of cure of crosslinked resins and compositions resulting therefrom
JPS51109999A (en) * 1975-03-25 1976-09-29 Sumitomo Electric Industries EHOKISHIJUSHINOKOKAHOHO
US4160064A (en) * 1977-06-15 1979-07-03 Theodore R. Flint Epoxy adhesive sealant
US4164492A (en) * 1978-03-14 1979-08-14 Alco Standard Corporation Novel catalyst for curing polyester resins and method for determining the degree of cure in polyester and epoxy resin systems
CH665483A5 (en) * 1985-11-22 1988-05-13 Coltene Ag METHOD FOR CONTROLLING THE HOMOGENEOUS MIXING OF A HAIRABLE MATERIAL AND A HARDENABLE MASS FOR CARRYING OUT THE METHOD.
FR2630743B1 (en) * 1988-04-29 1990-08-31 Gosselin Claude METHOD FOR SEALING BY INJECTION OF AN ACRYLAMIDE-BASED MIXTURE AND CORRESPONDING MIXTURE
US5607644A (en) * 1993-06-10 1997-03-04 Optical Sensors Incorporated Optical sensor for the measurement of pH in a fluid, and related sensing compositions and methods

Also Published As

Publication number Publication date
WO1998042762A1 (en) 1998-10-01
TW496888B (en) 2002-08-01
GB9706223D0 (en) 1997-05-14
DE69814604D1 (en) 2003-06-18
DE69814604T2 (en) 2004-04-29
CA2284841A1 (en) 1998-10-01
EP0970133A1 (en) 2000-01-12
EP0970133B1 (en) 2003-05-14
JP2001518973A (en) 2001-10-16
ZA982513B (en) 1998-09-28
US6060544A (en) 2000-05-09
ID22634A (en) 1999-12-02
ATE240358T1 (en) 2003-05-15

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